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BOC-Ala-Gly-OBzl → (S)-2-(2-((tert-Butoxycarbonyl)amino)propanamido)acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | BOC-Ala-Gly-OBzl | HCID 10980600 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | (S)-2-(2-((tert-Butoxycarbonyl)amino)propanamido)acetic acid | HCID 192414 | 87.5% |
反応手順
VII (16.97 g, 50 mmol) was taken in glacial acetic acid (170 ml) and hydrogenated overnight in the presence of 10% Pd/C (1.7 g) as catalyst at 40 psi. The catalyst was filtered with the aid of celite and solvent removed under reduced pressure. The residue was taken in satd. NaHCO3 solution, extracted with EtOAC (3×), cooled, acidified to pH 2.0 and re-extracted with EtOAC (3×). The combined EtOAC extracts were washed with satd. NaCl, and concentrated under reduced pressure. The residue was triturated with EtOAC: Pet. ether (1:1) and the precipitate obtained was filtered, washed with pet. ether and dried (10.9 g, yield: 87.5%), Rf4 0 52. Anal Calcd. for C10H18N2O5 .1/2H2O: C 46.50, H 7.41, N 10.84%. Found: C 46.64, H 7.41, N 10.84%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04976734 |
| 出典データセット | uspto-grants-1990_12 |
| ORD ID | ord-c65831c474ae4d56aa4733f535f28904 |
| 出典メモ | uspto-grants-1990_12 |